1、Designation: D4451 02 (Reapproved 2014)Standard Test Method forPigment Content of Paints by Low-Temperature Ashing1This standard is issued under the fixed designation D4451; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the pigment content of paintsand several traffic marking materials (thermoplastic and pre-f
3、ormed tape) by low-temperature furnace ashing. Some organicpigments may be lost by this method and some water ormoisture contained in pigments will be lost.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard do
4、es not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Sta
5、ndards:2D3723 Test Method for Pigment Content of Water-EmulsionPaints by Low-Temperature AshingE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals (Withdrawn 2009)33. Summary of Test Method3.1 The specimen is transferred to a tar
6、ed porcelain dish,dried (if necessary) at 105C, and heated on a burner. The dishand specimen are transferred to a muffle furnace and heated at450C. The dish and specimen are reweighed and the pigment(ash) content calculated.4. Apparatus4.1 Muffle Furnace, maintained at 450C 6 25C.4.2 Circulating Ove
7、n, maintained at 105C 6 2C.4.3 Porcelain Dishes, 90-mm diameter.4.4 Plastic Disposable Syringe, 10-mL capacity.4.5 Burner, meker type.5. Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the s
8、pecifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.45.2 Toluene.6. Procedure6.1 Liquid-Paint:6.1.1 Mix the sample until homogeneous, preferably on amechanical shaker. If air bubbles become entrapped in thepaint, stir it by
9、hand.6.1.2 Draw slightly more than 10 g of the paint under testinto a 10-mL syringe and weigh to 0.1 mg. Transfer about 5 mLtoluene to a porcelain dish tared with a paper clip for use as astirrer. Add 10 g of the material into the toluene. Reweigh thesyringe to 0.1 mg and calculate the specimen weig
10、ht. Mix wellon a magnetic stirrer. Place the dish in the oven at 105C for 30min.6.1.3 Remove and heat at the lowest temperature possibleover a meker burner in a fume hood. Do not leave the dish onthe burner after the flame has subsided. Transfer to the mufflefurnace and proceed as in 6.4.6.2 Preform
11、ed Traffc Marking TapeCut about a 10-gsquare of the product. Remove the adhesive by pulling it off orby using an appropriate solvent. Save the beads that areknocked off by this process and weigh with the tape. Dry thespecimen for 30 min at 105C to remove the solvent. Cool ina desiccator. Weigh the s
12、pecimen along with the loose beads to0.1 mg into a tared porcelain dish. Heat in a fume hood at thelowest temperature of a meker burner in a furnace hood until1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct
13、 responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved July 1, 2014. Published July 2014. Originally approvedin 1985. Last previous edition approved in 2008 as D4451 02 (2008). DOI:10.1520/D4451-02R14.2For referenced ASTM standards, visit th
14、e ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Reagent Chemical
15、s, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Fo
16、rmulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1the material catches fire. Do not leave the dish on the burnerafter the flame has subsided. Transfer to the muffle furna
17、ce andproceed as in 6.4.6.3 Thermoplastic Traffc Marking MaterialThis materialmay be delivered in block or powdered form. Transfer about400 g of the sample to a quart container and heat in a forceddraft oven at 400F until completely melted (may take as longas 4 h). Stir vigorously until well mixed.
18、Pour about 10 g of thesample into an aluminum dish and let it cool. Remove the 10g wafer from the aluminum dish and weigh to 0.1 mg. Transferto a tared porcelain dish. Heat the dish at the lowest tempera-ture of a meker burner in a fume hood until the specimencatches fire. Do not leave the dish on t
19、he burner after the flamehas subsided. Transfer to a muffle furnace and proceed as in6.4.6.4 Place the porcelain dish in a muffle furnace in a fumehood at 450C (see Test Method D3723). Heat overnight oruntil no further carbonaceous material is noted. Cool in adesiccator and reweigh the dish plus the
20、 residue to 0.1 mg.Calculate the residue as percent pigment or, in the case ofthermoplastic material and preformed tape, as pigment andbeads.7. Calculation7.1 Calculate the percent pigment, P, as follows:P 5 C 2 A/S 3100 (1)where:C = weight of dish and specimen after ignition in furnace, g,A = weigh
21、t of dish alone, g, andS = specimen weight used, g.8. Precision8.1 The precision estimates are based on an interlaboratorystudy in which one operator in 7 different laboratories analyzedin duplicate on two days six samples of commercial wholepaint or thermoplastic material containing 50 to 80 % pigm
22、ent.The results were analyzed statistically in accordance withPractice E180 and the within-laboratory coefficient of variationwas found to be 0.10 % relative at 36 df and the between-laboratories coefficient of variation 0.25 % relative at 30 df.Based on these coefficients the following criteria sho
23、uld beused for judging the acceptability of results at the 95 %confidence level:8.1.1 RepeatabilityTwo results, each the mean of dupli-cate determinations, obtained by the same operator on differentdays should be considered suspect if they differ by more than0.28 % relative.8.1.2 ReproducibilityTwo
24、results, each the mean of dupli-cate determinations, obtained by operators in different labora-tories should be considered suspect if they differ by more than0.72 % relative.9. Bias9.1 Bias cannot be determined because there are no stan-dards for pigment content of paints.10. Keywords10.1 ignition;
25、low temperature ashing; pigment; pigmentcontent of paintsASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such paten
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28、aring you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standar
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